CN107290460A - Diethylstilbestrol in a kind of beef and mutton, estradiol, the assay method of oestradiol benzoate and Estradiol Valerate estrogen residual quantity - Google Patents
Diethylstilbestrol in a kind of beef and mutton, estradiol, the assay method of oestradiol benzoate and Estradiol Valerate estrogen residual quantity Download PDFInfo
- Publication number
- CN107290460A CN107290460A CN201710488480.4A CN201710488480A CN107290460A CN 107290460 A CN107290460 A CN 107290460A CN 201710488480 A CN201710488480 A CN 201710488480A CN 107290460 A CN107290460 A CN 107290460A
- Authority
- CN
- China
- Prior art keywords
- estradiol
- diethylstilbestrol
- beef
- sample
- mutton
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Biological Materials (AREA)
- Steroid Compounds (AREA)
Abstract
The invention discloses the assay method of diethylstilbestrol in a kind of beef and mutton, estradiol, oestradiol benzoate and Estradiol Valerate estrogen residual quantity, including 1）Prepare mobile phase, chromatographic condition is set；2）Preparation, the test sample processing of standard items stock solution；3）The preparation of mixed sample；4）Linear regression analysis；5）The determination step of estrogen content in test sample.This method can detect the residual quantity of 4 kinds of estrogen in beef and mutton simultaneously, with detection limit is low, sensitivity is high, quick, result easy to operate accurately and reliably, testing conditions limit less advantage, with very big generalization, other hormone medicines are equally applicable to.
Description
Technical field
The invention belongs to measurement techniques for quality detection of meat detection technique field, in particular it relates to four kinds of estrogen residuals in a kind of beef and mutton
The assay method of amount.
Background technology
Currently, China's food-safety problem is of great interest because of " melamine " event in Sanlu milk powder.Except food
Maliciously add outer in processing, the chemical substance polluted in food more comes from animal feed used in nursing livestock and poultry, controlled
Sick used residue of veterinary drug and the growth regulator that accelerates the ripening used in plant etc..
Application of the hormone medicine in cattle and sheep industry can show the reproductive performance for improving cattle and sheep, and immunocastration, height is raised
Expect remuneration, promote growth, improve cattle and sheep meat, promote the output of milk etc. of lactation cattle and sheep.The beef and mutton that we eat is not yet
It is evitable to have estrogen residual, and these hormones will can induce canceration by food chain in people's cylinder accumulation, to reproduction
Influence is brought with the system such as nerve, serious environmental problem is also resulted in.The possibility that women obtains uterine cancer can also be increased, make genital tract
Produce inflammation, women is developed in advance, genital orgnas,male is occurred exception and lesion, and women with breast cancer and endometrium it is different
Position incidence rises, therefore, and the monitoring to beef and mutton is also to ensure one of safe measure.But at present in national standard only
The detection method of diethylstilbestrol, and remaining estrogen without clear and definite assay method.
The content of the invention
The invention aims to solve the above problems, there is provided diethylstilbestrol, estradiol, benzoic acid in a kind of beef and mutton
The assay method of estradiol and Estradiol Valerate estrogen residual quantity.
The purpose of the present invention is implemented by the following technical programs：
Diethylstilbestrol in a kind of beef and mutton, estradiol, the measure side of oestradiol benzoate and Estradiol Valerate estrogen residual quantity
Method, comprises the following steps：
1）Prepare mobile phase, chromatographic condition is set
Mobile phase：Methanol：Disodium phosphate soln volume ratio 80:20；
Chromatographic condition：Detection wavelength 210-400nm, flow velocity is 1.0ml/min, column temperature：40 DEG C, sample size is 10 μ l；
2）Preparation, the test sample processing of standard items stock solution
1. each 50mg of standard items of diethylstilbestrol, estradiol, oestradiol benzoate and Estradiol Valerate is weighed, is settled to respectively
50ml, is made 1.0mg/ml standard items stock solutions, standby；
2. weigh for examination beef and mutton sample, ultrasonic extraction-centrifugally operated twice is carried out with methanol, take the supernatant after centrifugation twice
Add methanol after being evaporated, machine in test sample treatment fluid, preparation is made in filtering；
3）The preparation of mixed sample
2.5ml steps 2 are drawn respectively）Obtained diethylstilbestrol, estradiol, oestradiol benzoate and Estradiol Valerate standard reserve
Liquid is simultaneously mixed, then it is 0.4mg/ml, 0.5mg/ml, 1.0mg/ml, system that mixed liquor is diluted into estrogen concentrations respectively with methanol
It is standby into mixed sample；
4）Linear regression analysis
By step 2）The single standard items stock solution of obtained estradiol, diethylstilbestrol, oestradiol benzoate and Estradiol Valerate
Filtering, with step 1）Condition be implanted sequentially in HPLC, according to the appearance time of standard items carry out it is qualitative, then by step 3）
0.4mg/ml, 0.5mg/ml, 1.0mg/ml for arriving mixed sample filtering, with step 1）Condition be implanted sequentially in HPLC, with 4
Plant mixed target peak area ratio and carry out linear regression analysis with its mass concentration, obtain 4 kinds of mixed target equations of linear regression；
5）The measure of estrogen content in test sample
By step 2）Obtained test sample treatment fluid is with step 1）Condition injection HPLC in, with peak area, by step 4）Obtain
Equation of linear regression calculate diethylstilbestrol in test sample treatment fluid, estradiol, oestradiol benzoate and Estradiol Valerate and contain
Amount, is then calculated for trying diethylstilbestrol in beef and mutton sample, estradiol, oestradiol benzoate and the residual quantity of Estradiol Valerate.
Further, the step 1）In, the concentration of the disodium phosphate soln is 0.043mol/l；
Chromatographic column type is：C18, ODS5 μm, 150 × 4mm；
The Detection wavelength is preferably 280nm.
Further, the step 2）In, the specific preparation method of the test sample treatment fluid is：
Weigh and crush sample 5.0g for examination beef and mutton, be put into 20ml centrifuge tube with cover, plus methanol 10.0ml, ultrasonic extraction
20min, 10min is centrifuged with 10000 turns/min, is removed and is added 10.0ml methanol in supernatant, residue again, then ultrasonic extraction 20min
, 10 min are centrifuged with 10000 turns/min, merge supernatant, in 80 DEG C of water bath methods, with 24ml methanol dissolved residues, through 0.22 μ
The disposable organic membrane filtrations of m, obtain test sample treatment fluid.
Further, the step 4）In, the filter membrane used during filtering is 0.45 μm of organic film.
Further, the step 5）In, for examination beef and mutton sample in diethylstilbestrol, estradiol, oestradiol benzoate and
The residual quantity computational methods of Estradiol Valerate are as follows：
X=V1C/mV2；
In formula：
X：The content mg/kg of a certain estrogen in sample；
C：The content ng of a certain estrogen obtained according to equation of linear regression；
V1：The final volume of dissolution ml of sample；
V2：Sampling volume μ l；
m：Sample quality g.
The invention has the advantages that：
Diethylstilbestrol, estradiol, oestradiol benzoate and Estradiol Valerate estrogen residual quantity in the beef and mutton that the present invention is provided
Assay method, the residual quantity of 4 kinds of estrogen in beef and mutton can be detected simultaneously, with detection limit is low, sensitivity is high, operation is simple
Just quick, result accurately and reliably, testing conditions limit less advantage, with very big generalization, be equally applicable to its separate excitation
Plain class medicine.
Brief description of the drawings
Fig. 1 is the mixed sample collection of illustrative plates of 4 kinds of estrogen；
Fig. 2 is the spectrum of singly marking on a map of estradiol；
Fig. 3 is the spectrum of singly marking on a map of diethylstilbestrol；
Fig. 4 is the spectrum of singly marking on a map of Estradiol Valerate；
Fig. 5 is the spectrum of singly marking on a map of oestradiol benzoate.
Embodiment
In order to more protrude the objects, technical solutions and advantages of the present invention, with the following Examples, the present invention is entered to advance
One step illustrates, but does not therefore limit the present invention within scope of embodiments.
Embodiment 1
1 material and method
1.1 material
1.1.1 reagent
Methanol, chromatographically pure, Chemical Reagent Co., Ltd., Sinopharm Group, Shanghai；
Sodium dihydrogen phosphate（NaH2PO4·2H2O）：Chemical Reagent Co., Ltd., Sinopharm Group, Shanghai；
0.043mol/l sodium dihydrogen phosphates：3.4g sodium dihydrogen phosphate（NaH2PO4·2H2O）It is dissolved in water and constant volume is in 500ml
Obtained in volumetric flask.
1.1.2 standard items
Diethylstilbestrol standard items：SIGMA-ALORICH, product of USA；
Estradiol standard items：SIGMA-ALORICH, product of Germany；
Oestradiol benzoate standard items：Nat'l Pharmaceutical ＆ Biological Products Control Institute；
Estradiol Valerate standard items：Nat'l Pharmaceutical ＆ Biological Products Control Institute.
Diethylstilbestrol, estradiol, the preparation side of oestradiol benzoate and Estradiol Valerate Standard Reserving Solution and mixed sample
Method：
Precision weighs 50mg diethylstilbestrols, estradiol, oestradiol benzoate and Estradiol Valerate standard items, and methanol constant volume is used respectively
In 50ml volumetric flasks, that is, each single target storing solution is obtained for 1mg/ml；Then 2.5ml diethylstilbestrols, female two are drawn respectively
Alcohol, oestradiol benzoate and the mixing of Estradiol Valerate Standard Reserving Solution, again with methanol are diluted to 0.4mg/ml, 0.5mg/ respectively
Ml, 1.0mg/ml, are stored in standby in refrigerator.
1.2 method
1.2.1 pre-treating method
Respectively in Lanzhou City, Gansu Province, Jingyuan County, Lin Xiazhou, 20 parts of meat samples of Zhangye Prefecture's collection, Lanzhou, Zhangye Prefecture
Gather 20 parts of beef sample.
Sample-pretreating method：Crushing sample 5.0g is weighed, is put into 20ml centrifuge tube with cover, plus methanol 10.0ml, surpass
Sound extracts 20min, centrifuges 10min（10000 turns/min）, remove supernatant.Add 10.0ml methanol, then ultrasonic extraction in residue again
20min, centrifuges 10min（10000 turns/min）, merge supernatant in 80 DEG C of water bath methods, with 24ml methanol dissolved residues, warp
Machine in 0.22 μm of disposable organic membrane filtration, preparation.
1.2.2 instrument and condition
Waters e2695 high performance liquid chromatographs, equipped with 2998 PAD detectors；Ultrasonic cleaner；Chromatographic column：C18,
ODS5 μm, 150 × 4mm；Mobile phase：Methanol：Disodium phosphate soln（0.043mol/l）=80:20；Flow velocity：1.0ml/min；
Column temperature：40℃；Detection wavelength：280nm.The single of diethylstilbestrol, estradiol, oestradiol benzoate and Estradiol Valerate is taken respectively
Standard items and 0.4mg/ml, 0.5 mg/ml, 1.0 mg/ml mixed sample take 10 μ through 0.45 μm of organic membrane filtration
L is implanted sequentially in HPLC, first qualitative with the appearance time of standard items, then with mixed sample, according to 4 kinds of mixed target peak area ratios with
Its mass concentration carries out linear regression analysis, obtains equation of linear regression.
1.2.3 calculation formula
X=V1C/mV2；
In formula：
X：The content (mg/kg) of a certain estrogen in sample；
C：The content of a certain estrogen obtained according to equation of linear regression（ng）；
V1：The final volume of dissolution of sample（ml）；
V2：Sampling volume（μl）；
m：Sample quality（g）.
2 results
The mixed spectrum of marking on a map of 4 kinds of estrogen is shown in Fig. 1, and estradiol, diethylstilbestrol, Estradiol Valerate, oestradiol benzoate list spectrum of marking on a map are shown in
Fig. 2-5.
The testing result of 4 kinds of estrogen residual quantities is shown in Table 1 in beef and mutton sample.
The testing result of 4 kinds of estrogen residual quantities in the beef and mutton sample of table 1
Note：" -- " represents not detect, and detected level unit is mg/kg, and all samples do not detect estrogen during primary detection, then
Mark-on test is carried out to Lanzhou, Linxia state meat samples and Lanzhou beef sample.
By table 1, estrogen residual is not detected in the local beef and mutton sample of 6 determined, during primary detection, so
Afterwards in Lanzhou and Linxia state meat samples, Lanzhou beef sample carry out mark-on detection, while detect diethylstilbestrol, it is female
In glycol, 4 kinds of estrogen of oestradiol benzoate and Estradiol Valerate, Lanzhou beef sample also simultaneously detect above-mentioned 4 kinds it is female
Hormone, illustrates that the method for the present invention is capable of detecting when the estrogen remained in beef and mutton.
3 conditions are selected
The selection of 3.1 mobile phases
Mobile phase is a most important step in chromatographic isolation, is directly connected to the sensitivity of analysis, detection limit, can decide by
The component of sample is separated one by one.Present invention methanol, the solvent of 0.043mol/l sodium dihydrogen phosphate different ratios enter
Experiment is gone, with methanol：Disodium phosphate soln=40:60th, methanol：Disodium phosphate soln=50:50th, methanol：Phosphoric acid hydrogen two
Sodium solution=70:30th, methanol：Disodium phosphate soln=80:20th, methanol：Disodium phosphate soln=90:10 grade different proportions
Mobile phase is tested.As a result show：With methanol：Disodium phosphate soln=80:20 be mobile phase, and separating effect is preferable.
The selection of 3.2 flow velocitys
The size of flow velocity directly affects pressure, sample each component separating effect and the appearance time of chromatographic column and system.In flowing
After mutually determining, the flow velocity of selection optimal separation degree and most short disengaging time, flow velocity is too small, and appearance time is oversize, and flow velocity is too big,
The pressure of system is too high, easily causes column cap to collapse.The application uses 1.0ml/min flow velocity.
The selection of 3.3 column temperatures
Column temperature is to influence one of factor of sample component separating degree.Prior art passes through mostly using 30 DEG C or room temperature as column temperature
Tested respectively with 30 DEG C, room temperature and 40 DEG C, as a result 40 DEG C of separating effect is preferable, therefore column temperature of the present invention uses 40 DEG C.
The selection of 3.4 wavelength：
Using the 3D passages of PAD detectors, search, found in 230nm and 280nm two in 210-400nm visible-range
Individual wavelength has preferable absorption, then finds separating degree of the separating degree compared with 230nm wavelength under 280nm wavelength with standard control
It is good, therefore it is used as wavelength from 280nm.
3.5 the inventive method ranges of linearity, correlation and detection limit experiment, as a result as shown in table 2.
The range of linearity of table 2, correlation and detection limit
3.6 precision test：
With the μ l of 1.0mg/ml mark-on sample extracting solutions sample introduction 10,6 analyses of sample introduction, its peak area, coefficient of variation result such as table 3
It is shown.
34 kinds of component peak areas of table（Area）The precision result of measure
3.7 accuracy test：
Using meat samples as sample, 3 levels of addition mix the mapping rate of recovery, as a result as shown in table 4.
The sample recovery of standard addition result of table 4
By table 4, recovery of standard addition scope is 85.96-101.56%.
By above-mentioned experiment, method detection limit of the invention is low compared with other method, and sensitivity is high, with higher essence
Density and the degree of accuracy.The instrument that the method for the present invention is used is more universal, and common lab can just possess, and 4 can be detected simultaneously
Estrogen is planted, with very big generalization.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, although with reference to foregoing reality
Apply example the present invention is described in detail, for those skilled in the art, it still can be to foregoing each implementation
Technical scheme described in example is modified, or carries out equivalent substitution to which part technical characteristic.All essences in the present invention
God is with principle, and any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.
Claims (5)
1. diethylstilbestrol in a kind of beef and mutton, estradiol, the measure of oestradiol benzoate and Estradiol Valerate estrogen residual quantity
Method, it is characterised in that comprise the following steps：
1）Prepare mobile phase, chromatographic condition is set
Mobile phase：Methanol：Disodium phosphate soln volume ratio 80:20；
Chromatographic condition：Detection wavelength 210-400nm, flow velocity is 1.0ml/min, column temperature：40 DEG C, sample size is 10 μ l；
2）Preparation, the test sample processing of standard items stock solution
1. each 50mg of standard items of diethylstilbestrol, estradiol, oestradiol benzoate and Estradiol Valerate is weighed, is settled to respectively
50ml, is made 1.0mg/ml standard items stock solutions, standby；
2. weigh for examination beef and mutton sample, ultrasonic extraction-centrifugally operated twice is carried out with methanol, take the supernatant after centrifugation twice
Add methanol after being evaporated, machine in test sample treatment fluid, preparation is made in filtering；
3）The preparation of mixed sample
2.5ml steps 2 are drawn respectively）Obtained diethylstilbestrol, estradiol, oestradiol benzoate and Estradiol Valerate standard reserve
Liquid is simultaneously mixed, then it is 0.4mg/ml, 0.5mg/ml, 1.0mg/ml, system that mixed liquor is diluted into estrogen concentrations respectively with methanol
It is standby into mixed sample；
4）Linear regression analysis
By step 2）The single standard items stock solution of obtained estradiol, diethylstilbestrol, oestradiol benzoate and Estradiol Valerate
Filtering, with step 1）Condition be implanted sequentially in HPLC, according to the appearance time of standard items carry out it is qualitative, then by step 3）
0.4mg/ml, 0.5mg/ml, 1.0mg/ml for arriving mixed sample filtering, with step 1）Condition be implanted sequentially in HPLC, with 4
Plant mixed target peak area ratio and carry out linear regression analysis with its mass concentration, obtain 4 kinds of mixed target equations of linear regression；
5）The measure of estrogen content in test sample
By step 2）Obtained test sample treatment fluid is with step 1）Condition injection HPLC in, with peak area, by step 4）Obtain
Equation of linear regression calculate diethylstilbestrol in test sample treatment fluid, estradiol, oestradiol benzoate and Estradiol Valerate and contain
Amount, is then calculated for trying diethylstilbestrol in beef and mutton sample, estradiol, oestradiol benzoate and the residual quantity of Estradiol Valerate.
2. diethylstilbestrol, estradiol, oestradiol benzoate and Estradiol Valerate are female sharp in beef and mutton according to claim 1
The assay method of plain residual quantity, it is characterised in that the step 1）In, the concentration of the disodium phosphate soln is
0.043mol/l；
Chromatographic column type is：C18, ODS5 μm, 150 × 4mm；
The Detection wavelength is preferably 280nm.
3. diethylstilbestrol, estradiol, oestradiol benzoate and Estradiol Valerate are female sharp in beef and mutton according to claim 1
The assay method of plain residual quantity, it is characterised in that the step 2）In, the specific preparation method of the test sample treatment fluid is：
Weigh and crush sample 5.0g for examination beef and mutton, be put into 20ml centrifuge tube with cover, plus methanol 10.0ml, ultrasonic extraction
20min, 10min is centrifuged with 10000 turns/min, is removed and is added 10.0ml methanol in supernatant, residue again, then ultrasonic extraction 20min
, 10 min are centrifuged with 10000 turns/min, merge supernatant, in 80 DEG C of water bath methods, with 24ml methanol dissolved residues, through 0.22 μ
The disposable organic membrane filtrations of m, obtain test sample treatment fluid.
4. diethylstilbestrol, estradiol, oestradiol benzoate and Estradiol Valerate are female sharp in beef and mutton according to claim 1
The assay method of plain residual quantity, it is characterised in that the step 4）In, the filter membrane used during filtering is 0.45 μm of organic film.
5. diethylstilbestrol, estradiol, oestradiol benzoate and Estradiol Valerate are female sharp in beef and mutton according to claim 1
The assay method of plain residual quantity, it is characterised in that the step 5）In, for diethylstilbestrol, estradiol, benzene in examination beef and mutton sample
The residual quantity computational methods of formic acid estradiol and Estradiol Valerate are as follows：
X=V1C/mV2；
In formula：
X：The content mg/kg of a certain estrogen in sample；
C：The content ng of a certain estrogen obtained according to equation of linear regression；
V1：The final volume of dissolution ml of sample；
V2：Sampling volume μ l；
m：Sample quality g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710488480.4A CN107290460A (en) | 2017-06-23 | 2017-06-23 | Diethylstilbestrol in a kind of beef and mutton, estradiol, the assay method of oestradiol benzoate and Estradiol Valerate estrogen residual quantity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710488480.4A CN107290460A (en) | 2017-06-23 | 2017-06-23 | Diethylstilbestrol in a kind of beef and mutton, estradiol, the assay method of oestradiol benzoate and Estradiol Valerate estrogen residual quantity |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107290460A true CN107290460A (en) | 2017-10-24 |
Family
ID=60098536
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710488480.4A Pending CN107290460A (en) | 2017-06-23 | 2017-06-23 | Diethylstilbestrol in a kind of beef and mutton, estradiol, the assay method of oestradiol benzoate and Estradiol Valerate estrogen residual quantity |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107290460A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020224471A1 (en) * | 2019-05-05 | 2020-11-12 | 江南大学 | Pretreatment method for ultrasonic-assisted extraction of various steroid hormones in sediments |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103983708A (en) * | 2014-05-06 | 2014-08-13 | 中国农业科学院兰州畜牧与兽药研究所 | Method for simultaneous measurement of residual quantities of four estrogens in beef and mutton |
| CN106872621A (en) * | 2015-12-10 | 2017-06-20 | 国家食品安全风险评估中心 | The extraction and purification methods of Residual estrogenic in a kind of animality sample |
-
2017
- 2017-06-23 CN CN201710488480.4A patent/CN107290460A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103983708A (en) * | 2014-05-06 | 2014-08-13 | 中国农业科学院兰州畜牧与兽药研究所 | Method for simultaneous measurement of residual quantities of four estrogens in beef and mutton |
| CN106872621A (en) * | 2015-12-10 | 2017-06-20 | 国家食品安全风险评估中心 | The extraction and purification methods of Residual estrogenic in a kind of animality sample |
Non-Patent Citations (2)
| Title |
|---|
| 李维红等: "HPLC法同时测定牛羊肉中4种雌激素的残留量", 《黑龙江畜牧兽医》 * |
| 李维红等: "甘肃省市售牛羊肉中雌激素残留状况分析", 《湖北农业科学》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020224471A1 (en) * | 2019-05-05 | 2020-11-12 | 江南大学 | Pretreatment method for ultrasonic-assisted extraction of various steroid hormones in sediments |
| US11976093B2 (en) | 2019-05-05 | 2024-05-07 | Jiangnan University | Ultrasonic-assisted pretreatment method for extraction of multiple steroid hormones in sediment |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100507558C (en) | Method for checking organic phosphorus pesticide residue in animal milk | |
| CN106770769A (en) | A kind of method of various liposoluble vitamins in detection feed | |
| CN107677757A (en) | The method for determining vanillic aldehyde in food, methyl vanillin, Ethyl vanillin simultaneously | |
| CN107144661B (en) | Detection method that is a kind of while obtaining material composition and total antioxidant activity in Honeysuckle flower | |
| CN103822814A (en) | QuEChERS extraction method for poisonous substance extraction and application of QuEChERS extraction method | |
| CN105445390A (en) | Method for detecting residues of chloramphenicols in milk products | |
| CN101482511A (en) | Fast detection reagent for detecting methanal in food, and its method and reagent kit | |
| CN105116063B (en) | The multi-joint detection method of cephalosporins medicine residual in a kind of dairy product | |
| CN105527367A (en) | Detection method for antibiotic residues in meat products | |
| CN107290460A (en) | Diethylstilbestrol in a kind of beef and mutton, estradiol, the assay method of oestradiol benzoate and Estradiol Valerate estrogen residual quantity | |
| CN109633028A (en) | The detection method of spice additive in a kind of special medicine purposes formula food | |
| CN108614052A (en) | The method for detecting gelsemine in biological sample, koumine and hexa-gelsemicine simultaneously based on two-dimensional liquid chromatography | |
| CN101446574A (en) | LC-MS quantitative detection method for melamine and tricyanic acid in human urine | |
| CN103983708A (en) | Method for simultaneous measurement of residual quantities of four estrogens in beef and mutton | |
| CN110441445A (en) | A kind of construction method and flavones ingredient assay of cockscomb HPLC characteristic fingerprint pattern | |
| RU2633013C2 (en) | Method for levomycetin determination in fodders of animal origin using high-effective liquid chromatography | |
| CN108181402A (en) | The detection method of content of zearalenone in a kind of cereal | |
| Huggett et al. | Rapid micro-method for the measurement of paracetamol in blood plasma or serum using gas-liquid chromatography with flame-ionisation detection | |
| Banes et al. | The analysis of digitoxin tablets | |
| CN114034794A (en) | Method for determining multi-component content of heat-clearing and detoxifying oral liquid | |
| CN107102078A (en) | A kind of method of aflatoxin B1 in measure Gardenia Yellow | |
| Odam et al. | The determination of warfarin in animal tissues by electron-capture gas-liquid chromatography | |
| CN106918661A (en) | A kind of high-performance liquid chromatogram determination method for determining Ah Ti woods C content in Detection of Brazilian Propolis soft capsule | |
| CN108693274B (en) | Method for detecting triazole pesticide residues in white wine by combining solidification-floating dispersion liquid microextraction and HPLC | |
| CN102967682B (en) | Ganoderma lucidum spores oil or ganoderma lucidum spore powder or quality test method of preparation thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171024 |